HRID493503

反应详情

EQUATION

反应方程式

HRID 493503 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Triethylamine (9.76 mL, 70 mmol) was added under nitrogen to a solution of 4′-hydroxy-biphenyl-4-carboxylic acid (15.0 g, 70 mmol) in 200 mL of anhydrous DMF at room temperature. After stirring for 5 minutes potassium carbonate (58.0 g, 420 mmol) was added and the reaction stirred an additional 5 minutes. Iodomethane (26.0 mL, 420 mmol) was then added (exothermic reaction) and the reaction stirred overnight. The reaction was diluted with methylene chloride, extracted multiple times with water, dried (MgSO4) and the solvent removed under reduced pressure to give 4′-methoxy-biphenyl-4-carboxylic acid methyl ester (16.26 g, 96%) as a tan solid, mp 170-173° C. Elemental Analysis for C15H14O3: Calc'd: C, 74.36; H, 5.82; N, 0.00; Found: C, 73.97; H, 5.66; N, 0.03.

WORKUP

后处理

  1. additionwas added
  2. custom(exothermic reaction)
  3. stirringthe reaction stirred overnight
  4. extractionextracted multiple times with water
  5. dry with materialdried (MgSO4)
  6. customthe solvent removed under reduced pressure